CN105924371A - Extraction method of L-citrulline in seed melon, and preparation method of effervescent tablet - Google Patents
Extraction method of L-citrulline in seed melon, and preparation method of effervescent tablet Download PDFInfo
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- CN105924371A CN105924371A CN201610281991.4A CN201610281991A CN105924371A CN 105924371 A CN105924371 A CN 105924371A CN 201610281991 A CN201610281991 A CN 201610281991A CN 105924371 A CN105924371 A CN 105924371A
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- cit
- resin
- dried
- pvp
- cationic ion
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- 239000007938 effervescent tablet Substances 0.000 title claims abstract description 38
- 241000219112 Cucumis Species 0.000 title claims abstract description 34
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 title claims abstract description 28
- FJJCIZWZNKZHII-UHFFFAOYSA-N [4,6-bis(cyanoamino)-1,3,5-triazin-2-yl]cyanamide Chemical compound N#CNC1=NC(NC#N)=NC(NC#N)=N1 FJJCIZWZNKZHII-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title abstract description 20
- 238000000605 extraction Methods 0.000 title abstract description 6
- RHGKLRLOHDJJDR-BYPYZUCNSA-N L-citrulline Chemical compound NC(=O)NCCC[C@H]([NH3+])C([O-])=O RHGKLRLOHDJJDR-BYPYZUCNSA-N 0.000 title abstract 10
- 229960002173 citrulline Drugs 0.000 title abstract 5
- 238000000034 method Methods 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 239000002245 particle Substances 0.000 claims abstract description 33
- 239000003513 alkali Substances 0.000 claims abstract description 24
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 18
- 238000004821 distillation Methods 0.000 claims abstract description 15
- 235000005979 Citrus limon Nutrition 0.000 claims abstract description 12
- 244000131522 Citrus pyriformis Species 0.000 claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 11
- 230000008025 crystallization Effects 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000010828 elution Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 86
- 239000011347 resin Substances 0.000 claims description 59
- 229920005989 resin Polymers 0.000 claims description 59
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 51
- 239000003729 cation exchange resin Substances 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims description 25
- 239000003480 eluent Substances 0.000 claims description 23
- 239000008187 granular material Substances 0.000 claims description 23
- 239000003826 tablet Substances 0.000 claims description 22
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 20
- 229930195725 Mannitol Natural products 0.000 claims description 20
- 239000000594 mannitol Substances 0.000 claims description 20
- 235000010355 mannitol Nutrition 0.000 claims description 20
- 239000012528 membrane Substances 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 235000015165 citric acid Nutrition 0.000 claims description 16
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 15
- 238000001179 sorption measurement Methods 0.000 claims description 15
- 239000006228 supernatant Substances 0.000 claims description 15
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 239000013078 crystal Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 235000019441 ethanol Nutrition 0.000 claims description 11
- 239000004376 Sucralose Substances 0.000 claims description 9
- BAQAVOSOZGMPRM-QBMZZYIRSA-N sucralose Chemical compound O[C@@H]1[C@@H](O)[C@@H](Cl)[C@@H](CO)O[C@@H]1O[C@@]1(CCl)[C@@H](O)[C@H](O)[C@@H](CCl)O1 BAQAVOSOZGMPRM-QBMZZYIRSA-N 0.000 claims description 9
- 235000019408 sucralose Nutrition 0.000 claims description 9
- 239000004383 Steviol glycoside Substances 0.000 claims description 7
- 230000006837 decompression Effects 0.000 claims description 7
- 235000019411 steviol glycoside Nutrition 0.000 claims description 7
- 229930182488 steviol glycoside Natural products 0.000 claims description 7
- 150000008144 steviol glycosides Chemical class 0.000 claims description 7
- 235000019202 steviosides Nutrition 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 6
- 229960003511 macrogol Drugs 0.000 claims description 6
- FEMOMIGRRWSMCU-UHFFFAOYSA-N ninhydrin Chemical compound C1=CC=C2C(=O)C(O)(O)C(=O)C2=C1 FEMOMIGRRWSMCU-UHFFFAOYSA-N 0.000 claims description 6
- 239000004033 plastic Substances 0.000 claims description 6
- 229920003023 plastic Polymers 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 235000020985 whole grains Nutrition 0.000 claims description 6
- 238000001471 micro-filtration Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 3
- 238000005374 membrane filtration Methods 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 150000001768 cations Chemical class 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 14
- 239000002253 acid Substances 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 235000019605 sweet taste sensations Nutrition 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000003344 environmental pollutant Substances 0.000 abstract 1
- 231100000719 pollutant Toxicity 0.000 abstract 1
- 229940093429 polyethylene glycol 6000 Drugs 0.000 abstract 1
- 235000019614 sour taste Nutrition 0.000 abstract 1
- 239000000047 product Substances 0.000 description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 230000033228 biological regulation Effects 0.000 description 5
- 235000009508 confectionery Nutrition 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 238000005341 cation exchange Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 239000011122 softwood Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- DWNBOPVKNPVNQG-LURJTMIESA-N (2s)-4-hydroxy-2-(propylamino)butanoic acid Chemical compound CCCN[C@H](C(O)=O)CCO DWNBOPVKNPVNQG-LURJTMIESA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 3
- 108090000790 Enzymes Proteins 0.000 description 3
- ODKSFYDXXFIFQN-BYPYZUCNSA-N L-arginine Chemical compound OC(=O)[C@@H](N)CCCN=C(N)N ODKSFYDXXFIFQN-BYPYZUCNSA-N 0.000 description 3
- 229930064664 L-arginine Natural products 0.000 description 3
- 235000014852 L-arginine Nutrition 0.000 description 3
- 235000001014 amino acid Nutrition 0.000 description 3
- 150000001413 amino acids Chemical class 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
- 239000003456 ion exchange resin Substances 0.000 description 3
- 229920003303 ion-exchange polymer Polymers 0.000 description 3
- 235000019629 palatability Nutrition 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000005292 vacuum distillation Methods 0.000 description 3
- 238000003828 vacuum filtration Methods 0.000 description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- 241000219109 Citrullus Species 0.000 description 2
- 235000012828 Citrullus lanatus var citroides Nutrition 0.000 description 2
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 2
- 229930006000 Sucrose Natural products 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000003712 anti-aging effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 235000014633 carbohydrates Nutrition 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 235000008504 concentrate Nutrition 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 150000002338 glycosides Chemical class 0.000 description 2
- 239000008101 lactose Substances 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 238000004080 punching Methods 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000005720 sucrose Substances 0.000 description 2
- 235000000346 sugar Nutrition 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005550 wet granulation Methods 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 208000003351 Melanosis Diseases 0.000 description 1
- 239000008118 PEG 6000 Substances 0.000 description 1
- 229920002584 Polyethylene Glycol 6000 Polymers 0.000 description 1
- 241000353135 Psenopsis anomala Species 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000007884 disintegrant Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
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- 230000004151 fermentation Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002070 germicidal effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 235000014666 liquid concentrate Nutrition 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 208000017497 prostate disease Diseases 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 235000012976 tarts Nutrition 0.000 description 1
- -1 therefore Polymers 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C273/18—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of substituted ureas
- C07C273/189—Purification, separation, stabilisation, use of additives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/185—Acids; Anhydrides, halides or salts thereof, e.g. sulfur acids, imidic, hydrazonic or hydroximic acids
- A61K31/19—Carboxylic acids, e.g. valproic acid
- A61K31/195—Carboxylic acids, e.g. valproic acid having an amino group
- A61K31/197—Carboxylic acids, e.g. valproic acid having an amino group the amino and the carboxyl groups being attached to the same acyclic carbon chain, e.g. gamma-aminobutyric acid [GABA], beta-alanine, epsilon-aminocaproic acid or pantothenic acid
- A61K31/198—Alpha-amino acids, e.g. alanine or edetic acid [EDTA]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/0002—Galenical forms characterised by the drug release technique; Application systems commanded by energy
- A61K9/0007—Effervescent
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/20—Pills, tablets, discs, rods
- A61K9/2004—Excipients; Inactive ingredients
- A61K9/2022—Organic macromolecular compounds
- A61K9/2031—Organic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyethylene glycol, polyethylene oxide, poloxamers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/20—Pills, tablets, discs, rods
- A61K9/2095—Tabletting processes; Dosage units made by direct compression of powders or specially processed granules, by eliminating solvents, by melt-extrusion, by injection molding, by 3D printing
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses an extraction method of L-citrulline in seed melon. The method comprises the steps of ultrafiltration liquid preparation, column elution, reduced-pressure distillation and crystallization. The invention also discloses an application of L-citrulline extracted with the above method. Specifically, materials with needed weight are prepared into acid particles and alkali particles; the particles are dried, and a lemon essence is sprayed in; the particles are dried, and are well mixed with polyethylene glycol 6000; and the mixture is tableted, such that L-citrulline effervescent tablets are obtained. The extraction method provided by the invention has the advantages of simple preparation process, low cost, low energy consumption, and low waste and pollutant production. The effervescent tablets prepared with the extracted L-citrulline have the advantages of fast disintegration, good effervescent effect, good sweet and sour taste, and convenient application. With the methods provided by the invention, a novel approach for comprehensively developing and utilizing seed melons is provided.
Description
Technical field
The invention belongs to processing of farm products field, relate to the extraction side of Cit in a seed melon
Method and the preparation method of effervescent tablet.
Background technology
Seed melon is branch's kind of watermelon, relative to common edible class watermelon, the plantation of seed melon
To obtain melon seeds, melon pulp, melon skin are all abandoned in vain as refuse, serious waste of resources
While make peasants suffer huge economic loss, the most greatly hinder seed melon industry send out
Exhibition, thus comprehensive development and utilization seed melon is inevitable choice.
Cit in seed melon, is a kind of nonessential amino acid.At prevention and treatment prostate
Disease aspect, Cit has significantly effect, different from improving sexuality medicine, L-melon
Propylhomoserin can improve male's sexual and can be absorbed in blood completely.In human body, by
Being the precursor of synthesis L-arginine in Cit, Cit can be converted in many tissues
One-tenth L-arginine, and intestines and stomach and liver not metabolism Cit, the most do not induce essence hydracid enzyme to live
Property raise, therefore supplement Cit and can assist and treat the L-arginine relevant disease that causes of shortage
Sick.Additionally, Cit can be as anti-aging, the health products of raising immunity, it is possible to as
Skin care, wrinkle resistant, nti-freckle, anti-aging women cosmetics.
The method producing Cit at present is mainly fermentation method, enzyme process, synthetic method and extraction method,
The chemical method used in prior art or biological synthesis process, complex steps is relatively costly and there is enzyme
The complex processes such as method conversion, this process control is the most difficult, often contains substantial amounts of enantiomeric
Body D-citrulling；And existing extraction method includes squeezing, concentration, cation exchange, crystallization etc.
Step, all there is other amino acid and remain too high in these methods, product purity is the highest, produces big
The shortcomings such as amount sewage.
Summary of the invention
Goal of the invention: in order to overcome above-mentioned the deficiencies in the prior art, the present invention provides a seed melon
The extracting method of middle Cit, main purpose is to simplify preparation flow, reduces cost, saves
The energy.
Another object of the present invention is to provide the preparation of Cit effervescent tablet in a seed melon
Method.
Technical scheme: for realizing the first invention, the present invention provides Cit in a seed melon
Extracting method, comprises the steps:
1) ultrafiltrate is prepared: the seed melon melon pulp after removing seed is squeezed the juice, is centrifuged, is taken supernatant, will
Ultrafiltration after supernatant micro-filtrate membrane filtration, then concentrate, obtain ultrafiltrate；
2) upper prop wash-out: by ultrafiltrate pH value to 1.0-2.0, obtain upper prop liquid, upper prop liquid is led to
Enter cationic ion-exchange resin exchange adsorption citrulling, when in detection efflux, Cit quality is dense
Degree is with when in ultrafiltrate, Cit mass concentration is identical, and exchange adsorption is complete, then uses ammoniacal liquor
As eluant, eluent, eluting, wash-out terminal is eluate ninhydrin reaction for feminine gender, collects
Eluent；
3) decompression distillation: obtain inspissated juice after the distillation and concentration that reduced pressure by eluent；
4) crystallization: inspissated juice absolute ethyl alcohol is crystallized, repeats crystallization 2-3 time, freeze-drying
After Cit crystal.
Further, described microfiltration membranes is the Flat Membrane in 0.1-0.3um aperture, and ultrafiltration is chosen and retained
Molecular weight is the daltonian Flat Membrane of 5000-7000, and the ultrafiltration time is 20-80min；
In described ultrafiltrate, Cit mass concentration is 0.2-4.0mg/mL.
Further, described cationic ion-exchange resin is 001 × 7 type, HD-8 type or 732 types；
The column flow rate of crossing of described upper prop liquid is 3.6-7.2BV/h, the use of described cationic ion-exchange resin
Amount is 20-25ml；
The volume of described inspissated juice is the 1/5-2/3 of effluent volume；
Described inspissated juice and volume ratio 1:3-5 of absolute ethyl alcohol.
Further, the molar concentration of described ammoniacal liquor is 0.6-0.9mol/L, and elution flow rate is
3.6-7.2BV/h。
Further, described step 2) also include the step to cationic ion-exchange resin pretreatment before
Rapid: cationic ion-exchange resin is placed in plastic containers, rinse with clear water, be soaked in water resin
12-24h so that it is fully expand, then loads in post by cationic ion-exchange resin, uses cation
The HCl of the 4% of exchanger resin volume 3-6 times flows through resin bed with the speed of 1mL/min, instead
Rinse 3 to 5 times again；The most again with water washing resin from top to bottom, until efflux pH is 3-5；
Use the NaOH solution speed stream with 1mL/min of cationic ion-exchange resin volume 2-4 times 4% again
Crossing resin bed, being then washed to pH is 8-9, then with 2-4 times of cationic ion-exchange resin volume
The HCl solution of 4% flows through resin bed with the speed of 1mL/min, and being then washed to pH is 3-5,
Without Cl-?.
Further, a kind of Cit, is to prepare according to above-mentioned extracting method.
For realizing the second object of the present invention, the present invention provides Cit effervesce in a seed melon
The preparation method of sheet:
A kind of composition for effervescent tablet, including the component of following weight portion:
Cit 25-35 part, citric acid 17-21 part, mannitol 10-14 part, Sucralose
2-4 part, steviol glycoside 0.1-0.5 part, PVP-k30Ethanol solution A 4-6 part；
Sodium acid carbonate 14-17 part, mannitol 16-20 part, PVP-k30Ethanol B solution 5-9 part；
Lemon extract 0.6-1.0 part, Macrogol 6000 1.8-2.5 part；
Described Cit is selected from Cit described in claim 5；
Described PVP-k30Ethanol solution A be mass concentration be the PVP-k of 90%30Ethanol solution,
Described PVP-k30Ethanol B solution be mass concentration be the PVP-k of 20%30Ethanol solution.
Preferably, the method using above-mentioned composition to prepare effervescent tablet, comprise the steps:
1) by Cit, citric acid, mannitol, Sucralose, steviol glycoside, PVP-k30
Ethanol solution A is directly prepared into granulates after mixing, and is then dried granulates；
2) by sodium acid carbonate, mannitol and PVP-k30Ethanol B solution is directly made after mixing
Become alkali particle, be then dried alkali particle；
3) after granulates and the whole grain of alkali particle, spray into lemon extract, add polyethylene glycol after drying
6000, be mixed evenly, compressing tablet, effervescent tablet.
Preferably, described preparing during effervescent tablet temperature required for 18-30 DEG C, relative humidity is
30-48%.
Preferably, described step 1) in the temperature that is dried be 42-47 DEG C, the time being dried is
1.5-3.5h；Described step 2) in be dried temperature be 35-42 DEG C, be dried time be 8-12min；
Described step 3) in be dried temperature be 38-42 DEG C, be dried time be 0.8-1.2h.
The invention have the benefit that
1. the present invention selects through the ultrafiltrate concentrated as upper prop liquid, by concentration suitable for upper prop liquid
Can improve concentration, reduce the consumption of resin, reduce the volume that pregnant solution is collected, beneficially resource is returned
Receive, save the consumption of the energy.
2. the present invention is with seed melon discarded object as raw material, utilizes ultrafiltration and ion exchange resin method direct
Extracting citrulling from seed melon, technological process is short, and energy consumption is low, is suitable for industrialized production；Cause
In the supernatant extracted, the impurity such as various albumen, carbohydrate is more, for improving resin to Cit
Adsorbance, upper prop liquid is pre-processed by the present invention, it may be assumed that choosing aperture is 0.1-0.3um
Flat Membrane be that 5000-7000 is daltonian flat by choosing molecular cut off after supernatant suction filtration again
Plate film ultrafiltration, filters supernatant with milipore filter, reconciles after pH value obtains upper prop liquid and goes up
Ion exchange resin adsorbs, and can significantly improve resin separative efficiency, alleviate the pollution to resin,
Extend resin use the cycle, reduce investment outlay, and product purity can be improved, it is thus achieved that citrulling produce
Product do not contain harmful substance, can be directly used for food and medicine and produce.
3. the present invention selects soda acid to separate wet granulation technology, can effectively prevent acid in preparation process
Source and alkali source react, it is ensured that the stability of product in production process；Tableting processes is difficult to
Glutinous punching, energy slice smoothly, tablet is smooth clean and tidy, in faint yellow；Owing to Cit contains carboxylic
Base, so softwood processed should not be mixed with sodium acid carbonate, suitably prepares granulates together with citric acid,
Thus the present invention chooses citric acid and prepares granulates together with Cit；This preparation technology reappears
Property good, tablet quality is stable, the Cit Effervescent tablet disintegration of preparation rapidly, effervesce effect
Good, sour and sweet palatability, taking convenience.
Accompanying drawing explanation
Fig. 1 is that in the embodiment of the present invention, pH value affects figure to ion-exchange effect；
Fig. 2 is that in the embodiment of the present invention, upper column liquid concentration affects figure to resin adsorption performance；
Fig. 3 is in the embodiment of the present invention on exchanger resin, crosses column flow rate and exchanges Cit
That measures affects figure；
Fig. 4 is that in the embodiment of the present invention, eluent ammonia concn affects figure to elute effect.
Detailed description of the invention
By further illustrate technological means that the present invention taked by reaching predetermined goal of the invention and
Effect, below in conjunction with accompanying drawing and preferred embodiment, to the specific embodiment party according to the present patent application
Formula, step, technical characteristic and function thereof, effect, after describing in detail such as.
In one seed melon, the extracting method of Cit, comprises the steps:
1) ultrafiltrate is prepared: the seed melon melon pulp after removing seed is squeezed the juice, is centrifuged, is taken supernatant, will
Ultrafiltration after supernatant micro-filtrate membrane filtration, then concentrate, obtain ultrafiltrate, ultrafiltrate is concentrated；
2) upper prop wash-out: by ultrafiltrate pH value to 1.0-2.0, obtain upper prop liquid, upper prop liquid is led to
Enter cationic ion-exchange resin exchange adsorption citrulling, when in detection efflux, Cit quality is dense
Degree is with when in ultrafiltrate, Cit mass concentration is identical, and exchange adsorption is complete, then uses ammoniacal liquor
As eluant, eluent, eluting, wash-out terminal is eluate ninhydrin reaction for feminine gender, collects
Eluent；
3) decompression distillation: obtain inspissated juice after the distillation and concentration that reduced pressure by eluent；
4) crystallization: inspissated juice absolute ethyl alcohol is crystallized, repeats crystallization 2-3 time, freeze-drying
After Cit crystal.
The present invention regulates pH value after being concentrated by ultrafiltrate, obtains upper prop liquid, by micro-filtration and ultrafiltration
Remove in upper prop liquid the impurity such as various albumen, carbohydrate, improve the adsorbance of resin after upper prop, subtract
The light pollution to resin, extends resin and uses the cycle, improve product purity.
In the present invention, the pH value of upper prop liquid has two aspects to the impact of ion-exchange effect, on the one hand
It is the impact that resins exchange group is dissociated, is on the other hand to affect dissociating of adsorbed material；
So the pH value of upper prop liquid mainly affects dissociating of Cit；Take upper prop liquid 30mL respectively,
Concentration is the former extract of 0.9569mg/mL, adjusts different pH value with acidometer, adds 3g
Wet resin, shaking table Static Adsorption 4h, rotating speed is that 114r/min investigates different pH value to tree
The impact of fat static adsorbance, as it is shown in figure 1, adsorbance difference is little when pH is 1-2,
And adsorbance is maximum under this pH value, therefore to reach preferable adsorption effect, the present invention will
The pH value of upper prop liquid is adjusted to 1-2；Because the isoelectric point of Cit is 5.97, pH is 1-2
Just away from the isoelectric point of Cit, so basic positively charged, adsorbance is optimum, if extracting
Liquid pH is just in the range of 1-2, then extract need not regulate pH and gets final product direct upper prop.
In order to make citrulling have more preferable adsorbance in the present invention, cationic ion-exchange resin needs
Pretreatment, will be placed in plastic containers by resin, rinses with clear water, and be soaked in water resin 12-24
H so that it is fully expand, then loads in post by resin, with the HCl of the 4% of resin volume 5 times
Flow through resin bed with the speed of 1mL/min, repeatedly rinse 3 to 5 times；Use low pure water the most again
Washing resin from top to bottom, until efflux pH is about 4；Again with resin volume 3 times 4%
NaOH solution processes, and is then washed to alkalescence, then the HCl of 4% with 3 times of resin volumes
Solution processes, and is then washed to pH and is about 4, without Cl-?.
Preferably, described microfiltration membranes is the Flat Membrane in 0.1-0.3um aperture, and ultrafiltration is chosen and retained point
Son amount is the daltonian Flat Membrane of 5000-7000, and the ultrafiltration time is 20-80min；Described ultrafiltration
After liquid concentrates, Cit mass concentration is 0.2-4.0mg/mL.
It is more uniform that microfiltration membranes used in the present invention has aperture ratio, and porosity is high, takes off without medium
The features such as falling, quality is thin, and resistance is little, and filtering velocity is fast, the Flat Membrane using 0.1-0.3um aperture can
To be filtered to remove solid insoluble matter and most big molecule class impurity, use 5000-7000 afterwards
After daltonian flat membrane ultrafiltration, other materials such as microorganism, colloid can be removed.
In order to clearly go up the column liquid concentration impact on resin adsorption performance, compound concentration of the present invention divides
Be not 0.2392,04785,0.9569,1.1438,1.1798,1.8594,2.3359mg/mL
The each 30mL of Cit sample liquid, add 3g wet resin, shaking table Static Adsorption 4h,
Investigate the variable concentrations impact on resin static adsorbance, as in figure 2 it is shown, along with Cit
The increase of concentration, adsorbance increases accordingly, and this result matches with adsorption equilibrium theory, will be super
The suitable concentration of filtrate can improve concentration, reduces the volume that pregnant solution is collected, beneficially resource reclaim,
Save the consumption of the energy.Therefore, the present invention selects through the ultrafiltrate concentrated as upper prop liquor ratio
Advantageous.
Preferably, described cationic ion-exchange resin is 001 × 7 type, HD-8 type or 732 types, institute
The column flow rate of crossing stating upper prop liquid is 3.6-7.2BV/h.
In order to clearly cross the column flow rate impact on Cit exchange capacity, the present invention respectively takes 25mL
The cationic ion-exchange resin dress post pre-processed, with Cit concentration as 3.9685mg/mL
Post exchange crossed by extract, controlled post speed and is respectively 3.6BV/h, 5.4BV/h, 7.2BV/h,
In units of every 10mL, collected post liquid respectively, measure and wherein cross Cit concentration in post liquid,
Till in efflux, Cit concentration is 3.9685mg/mL, as it is shown on figure 3, along with
Crossing post flow velocity to increase, upper prop liquid used is long-pending to be reduced, cationic ion-exchange resin exchange L-melon ammonia
The amount of acid reduces.When flow velocity is 3.6BV/h, the exchange capacity of resin is 31.75mg/mL；
When flow velocity brings up to 7.2BV/h, its exchange capacity drops to 20.64mg/mL.Obviously, this
Relevant with Cit diffusion velocity in resin.Cationic ion-exchange resin and Cit
Exchange rate determines that, and Cit is continuous between solution and resin during crossing post
Being diffused, when column flow rate is less excessively, Cit can carry out sufficient ion friendship with resin
Changing, therefore, its exchange capacity is big；Increasing along with crossing column flow rate, Cit flows through exchange column
Time gradually decreases.If in extract, Cit concentration is higher, then part Cit comes
Carrying out ion-exchange reactions just by exchange column not as good as with resin, therefore, resin is to Cit
Exchange capacity reduce.
Preferably, the molar concentration of described ammoniacal liquor is 0.6-0.9mol/L, and elution flow rate is 3.6-7.2
BV/h。
The isoelectric point of Cit is 5.97, pH=1-2 just away from the isoelectric point of Cit,
Now Cit is attracted in resin with cationic form.The present invention selects ammoniacal liquor to be wash-out
Agent is because the aobvious alkalescence of ammoniacal liquor, creates alkaline environment, and now solution environmental pH is more than Cit
Isoelectric point, can be eluted out Cit from resin.Because amino acid is in alkalescence condition
Change of configuration is the most easily caused to lose physiologically active, so eluent can use decompression distillation
Mode removes eluant, eluent.Ammoniacal liquor is volatile, uses distillation under vacuum to be easy to remove ammonia after wash-out
Water, therefore select ammoniacal liquor as eluant, eluent.
The effect of wash-out can be directly affected as eluant, eluent, the concentration of eluant, eluent using ammoniacal liquor, as
Really eluant strength is higher, and eluting power is the strongest, and the impurity flow down from resin is the most a lot,
If eluant strength is the dilutest, then the volume collecting liquid will strengthen, and goes out peak smooth, during collection
Between can extend.The present invention take 10mLL-citrulling solution that loading concentration is 0.3968mol/L,
Amount of resin is the 732 type cationic ion-exchange resins dress posts of 20mL, with the ammoniacal liquor of variable concentrations (0.2,
0.6,1.0mol/L) it is eluant, eluent, control elution flow rate is 7.2BV/h, with every 10mL is
Unit collected post liquid respectively, measures the absorbance of efflux, is converted into Cit content.
With eluant, eluent volume as abscissa, stripping post liquid Cit content is that ordinate draws wash-out
Curve, compares the impact on wash-out effect of three different eluant strengths.As shown in Figure 4,1.0
Mol/L wash-out power is the strongest, and acquisition time is short, but the most in view of its outflow impurity, so this
The ammonia spirit of bright preferred 0.6mol/L, although collect the big of the long-pending relatively 1.0mol/L of liquid,
But it goes out peak unevenness.
The present invention also provides for the preparation method of Cit effervescent tablet in a seed melon, and the method is first
First providing a kind of composition for effervescent tablet, said composition includes the component of following weight portion:
Cit 25-35 part, citric acid 17-21 part, mannitol 10-14 part, Sucralose
2-4 part, steviol glycoside 0.1-0.5 part, PVP-k30Ethanol solution A 4-6 part；
Sodium acid carbonate 14-17 part, mannitol 16-20 part, PVP-k30Ethanol B solution 5-9 part；
Lemon extract 0.6-1.0 part, Macrogol 6000 1.8-2.5 part；
Cit is to be prepared from according to the extracting method of Cit in an aforesaid seed melon,
PVP-k30Ethanol solution A be mass concentration be the PVP-k of 90%30Ethanol solution, PVP-k30
Ethanol B solution be mass concentration be the PVP-k of 20%30Ethanol solution.
Prepare effervescent tablet to commonly use filler and have sucrose, lactose, soluble starch, mannitol etc.,
As filler sucrose, there is good compressibility and mouthfeel, but easily absorb moisture, be not suitable for sugar
Urine patient；And Cit contains primary amino radical, should not share, one with reduced sugars such as lactose
Maillard reaction can occur under fixed condition；Soluble starch, mouldability and compressibility are poor；Sweet
Dew alcohol is white crystalline powder, soluble in water, character torpescence, and sweet taste is tasty and refreshing, stable
Property good, be placed in air unchanged, mobility and compressibility are good, no hygroscopicity, are dried
Hurry up, done tablet smooth in appearance is attractive in appearance, further, since effervescent tablet preparation formulation limits, available
Filler scope fewer, through experiment investigation select mannitol as filler, indices
All meet regulation.
The mellow and full soft tart flavour of citric acid so that it is extensively favored as food additives, be
Current most widely used effervesce acid source, and the acid source such as tartaric acid, malic acid is equal in terms of mouthfeel
There is deficiency；Compared with sodium carbonate, sodium acid carbonate is the quickest with organic acid reaction, same amount feelings
Producing more carbon dioxide under condition, therefore, the present invention finally selects citric acid and carbonic acid
Hydrogen sodium makees gas-producing disintegrant, and the optimum proportioning both optimization and addition.
Effervescent tablet has certain requirement to solution appearance, and in Cit water, dissolubility is preferable, suitable
Preferably making water-soluble effervescent tablet, through experiment sieving, PEG 6000 is as lubricant, lubricant effect
Good, not sticking, solution clarification after effervesce, institute's tablet agent smooth surface rounding, the most easy to wear.
Compared with cellulose family adhesive, PVPk30Water can be dissolved in and can be dissolved in again ethanol, stickiness
Well, and do not affect the clarity of solution after the disintegration of tablet and disintegration, be chosen as the present invention
Adhesive, citric acid meets water and absorbs water the most immediately and get wet, and softwood is difficult to sieve, and particle easily becomes bar
Shape, therefore selects the ethanol of high concentration as wetting agent, can play preferable stickiness peptizaiton,
Prepare suitable softwood.
On the basis of this enforcement is listed in above-described embodiment, above-mentioned composition is used to prepare effervescent tablet
Method, comprises the steps:
1) by Cit, citric acid, mannitol, Sucralose, steviol glycoside, PVP-k30
Ethanol solution A is directly prepared into granulates after mixing, and is then dried granulates；
2) by sodium acid carbonate, mannitol and PVP-k30Ethanol B solution is directly made after mixing
Become alkali particle, be then dried alkali particle；
3) after granulates and the whole grain of alkali particle, spray into lemon extract, add polyethylene glycol after drying
6000, be mixed evenly, compressing tablet, effervescent tablet.
The preparation method of the present invention selects soda acid to separate wet granulation technology, can effectively prevent preparation
During acid source and alkali source react, it is ensured that the stability of product, compressing tablet in production process
Process is difficult to glutinous punching, energy slice smoothly, and tablet is smooth clean and tidy, in faint yellow；Due to L-melon ammonia
Acid is containing carboxyl, so softwood processed should not be mixed with sodium acid carbonate, and suitable together with citric acid
Preparing granulates, therefore the present invention selects citric acid to prepare granulates together with Cit；This
Method reappearance is good, and tablet quality is stable, the Cit Effervescent tablet disintegration of preparation rapidly,
Effervesce is effective, sour and sweet palatability, taking convenience.
On the basis of this enforcement is listed in above-described embodiment, prepare during effervescent tablet temperature required for 18-
30 DEG C, relative humidity is 30-48%.
Containing citric acid in effervescent tablet, hygroscopicity is strong, should strictly control the wettest of workshop
Degree and the storage requirement of material, prevent the moisture absorption.At room temperature 18-30 DEG C, the bar of relative humidity 48%
Under part, compressing tablet effect is preferable.According to Germicidal efficacy, to control relative humidity (RH) as 30-48%
It is preferred, otherwise chemical reaction likely can occur and produce bubble after the mixing of soda acid particle, thus
The outward appearance making tablet is rough, spottiness etc..
On the basis of this enforcement is listed in above-described embodiment, step 1) in the baking temperature of granulates be
40-50 DEG C, the time is 2-4h；Step 2) in the baking temperature of alkali particle be 40-50 DEG C, be dried
Time is 10-30min；Step 3) in be dried temperature be 38-42 DEG C, drying time is 0.8-1.2h.
During preparing Cit effervescent tablet, water content sour, alkali particle is critically important,
Relatively dry, and want the humidity in strictly controlled environment air, the otherwise easy moisture absorption, and
Pelletization wants fast.
The water content of particle can affect compressing tablet situation and store during the stability of product, therefore,
Need the moisture controlling in particle in suitable scope.Sodium acid carbonate is easily subject to more than 65 DEG C
Thermal decomposition, should control baking temperature less than 65 DEG C.It addition, the selection of drying time is the most critically important,
Drying time is oversize, and efficiency is low and energy resource consumption increases, and drying time is the shortest, and particle drying is not
Thoroughly, affect product quality, therefore, suitable drying time and temperature need to be selected to control particle
Moisture, the present invention chooses certain temperature and time and is separately dried granulates and alkali particle, as
Shown in Tables 1 and 2, granulates is at 40-50 DEG C, and under 2-4h drying condition, particle water content is equal
Less than 1.9%, alkali particle is at 40-50 DEG C, and under 10-30min drying condition, water content is below
1%, it addition, after spraying into lemon extract at a temperature of 38-42 DEG C, after being dried 0.8-1.2h, compressing tablet is equal
Phenomenon without sticking, institute's tablet agent hardness is moderate, unilateral bright and clean.From saving the energy and time cost
And the effect consideration that compressing tablet is best, preferred acid particle is dried 2h, alkali particle in 45 DEG C of temperature
In 45 DEG C of temperature, it is dried 20min, after spraying into lemon extract, at a temperature of 40 DEG C, is dried 1h.
Table 1 granulates drying condition
Table 2 alkali particle drying condition
Below by specific embodiment, the present invention is further illustrated.
Embodiment 1:
In one seed melon, the extracting method of Cit, comprises the steps:
1) ultrafiltrate is prepared: the seed melon melon pulp after removing seed is squeezed the juice, is centrifuged, is taken supernatant, will
Supernatant is with after the Flat Membrane vacuum filtration in 0.2um aperture, and choosing molecular cut off is 5000 roads
You flat membrane ultrafiltration 50min, then be concentrated in vacuo to Cit mass concentration and be
4.0mg/mL, obtains ultrafiltrate；
2) upper prop wash-out: the regulation of ultrafiltrate pH value is obtained upper prop liquid to 1.2, upper prop liquid is led to
Enter the 732 type cationic ion-exchange resin exchange adsorption citrulling that loadings is 20ml, cross column flow rate
For 7.2BV/h, in efflux Cit mass concentration be adsorb during 4.0mg/mL complete,
With the ammoniacal liquor wash-out that molar concentration is 0.6mol/L, elution flow rate is 7.2BV/h, elutes terminal
It is negative for eluate ninhydrin reaction, collects eluent；
3) decompression distillation: by eluent the 1/3 of vacuum distillation apparatus distillation and concentration to original volume
After inspissated juice；
4) crystallization: being crystallized by inspissated juice absolute ethyl alcohol, crystalline solid slowly separates out to nodeless mesh body
Being terminal during precipitation, the water that crystal quality is 3 times of crystal mass after filtration dissolves, then
Repeat to crystallize 2 times with absolute ethyl alcohol, after freeze-drying, obtain Cit crystal, anhydrous second used
Alcohol and volume ratio 4:1 of inspissated juice；
Step 2) to the step of cationic ion-exchange resin pretreatment be before: by cation exchange tree
Fat is placed in plastic containers, rinses with clear water, and be soaked in water resin 20h so that it is fully expands,
Then cationic ion-exchange resin is loaded in post, with the 4% of cationic ion-exchange resin volume 5 times
HCl flows through resin bed with the speed of 1mL/min, repeatedly rinses 4 times；The most again with water from upper
And lower washing resin, until efflux pH is 4；Again with cationic ion-exchange resin volume 3 times 4%
NaOH solution flow through resin bed with the speed of 1mL/min, being then washed to pH is 8, then
Flow through with the speed of 1mL/min with the HCl solution of the 4% of 3 times of cationic ion-exchange resin volumes
Resin bed, being then washed to pH is 4, without Cl-?.
In one seed melon, the preparation method of Cit effervescent tablet, comprises the steps:
1) take Cit 30g, citric acid 19.1g, mannitol 12.1g, Sucralose 1.5g,
Steviol glycoside 0.3g, mass concentration are the PVP-k of 90%30Ethanol solution 5g is direct after mixing
Make granulates, 45 DEG C of dry 2h；
2) take sodium acid carbonate 15.9g, mannitol 18.4g, mass concentration are the PVP-k of 20%30
Ethanol solution 7g, is directly prepared into alkali particle, 45 DEG C of dry 20min after mixing；
3) lemon extract 0.8g will be sprayed into after dried granulates, the whole grain of alkali particle, do for 40 DEG C
After dry 1h, add 2g Macrogol 6000, be mixed evenly, compressing tablet, finished product.
Preparing effervescent tablet temperature required is 25 DEG C, and relative humidity is 48%.
Embodiment 2:
In one seed melon, the extracting method of Cit, comprises the steps:
1) ultrafiltrate is prepared: the seed melon melon pulp after removing seed is squeezed the juice, is centrifuged, is taken supernatant, will
Supernatant is with after the Flat Membrane vacuum filtration in 0.1um aperture, and choosing molecular cut off is 7000 roads
You flat membrane ultrafiltration 20min, then be concentrated in vacuo to Cit mass concentration and be
3.0mg/mL, obtains ultrafiltrate；
2) upper prop wash-out: the regulation of ultrafiltrate pH value is obtained upper prop liquid to 2.0, upper prop liquid is led to
Enter 001 × 7 type cationic ion-exchange resin exchange adsorption citrulling that loadings is 25ml, cross post
Flow velocity is 3.6BV/h, in efflux Cit mass concentration be adsorb during 3.0mg/mL complete,
With the ammoniacal liquor wash-out that molar concentration is 0.9mol/L, elution flow rate is 3.6BV/h, elutes terminal
It is negative for eluate ninhydrin reaction, collects eluent；
3) decompression distillation: by eluent the 1/5 of vacuum distillation apparatus distillation and concentration to original volume
After inspissated juice；
4) crystallization: being crystallized by inspissated juice absolute ethyl alcohol, crystalline solid slowly separates out to nodeless mesh body
Being terminal during precipitation, the water that crystal quality is 2 times of crystal mass after filtration dissolves, then
Repeat to crystallize 3 times with absolute ethyl alcohol, after freeze-drying, obtain Cit crystal, anhydrous second used
Alcohol and volume ratio 3:1 of inspissated juice；
Step 2) to the step of cationic ion-exchange resin pretreatment be before: by cation exchange tree
Fat is placed in plastic containers, rinses with clear water, and be soaked in water resin 12h so that it is fully expands,
Then cationic ion-exchange resin is loaded in post, with the 4% of cationic ion-exchange resin volume 3 times
HCl flows through resin bed with the speed of 1mL/min, repeatedly rinses 3 times；The most again with water from upper
And lower washing resin, until efflux pH is 3；Again with cationic ion-exchange resin volume 2 times 4%
NaOH solution flow through resin bed with the speed of 1mL/min, being then washed to pH is 8, then
Flow through with the speed of 1mL/min with the HCl solution of the 4% of 2 times of cationic ion-exchange resin volumes
Resin bed, being then washed to pH is 3, without Cl-?.
In one seed melon, the preparation method of Cit effervescent tablet, comprises the steps:
1) Cit 25g, citric acid 21g, mannitol 10g, Sucralose 4g, sweet is taken
Synanthrin glycosides 0.1g, mass concentration are the PVP-k of 90%30Ethanol solution 4g directly makes after mixing
Become granulates, 42 DEG C of dry 1.5h；
2) take sodium acid carbonate 17g, mannitol 20g, mass concentration are the PVP-k of 20%30Ethanol
Solution 5g, is directly prepared into alkali particle, 42 DEG C of dry 8min after mixing；
3) lemon extract 1.0g will be sprayed into after dried granulates, the whole grain of alkali particle, do for 38 DEG C
After dry 1.2h, add 1.8g Macrogol 6000, be mixed evenly, compressing tablet, L-melon
Propylhomoserin effervescent tablet.
Preparing effervescent tablet temperature required is 18 DEG C, and relative humidity is 30%.
Embodiment 3:
In one seed melon, the extracting method of Cit, comprises the steps:
1) ultrafiltrate is prepared: the seed melon melon pulp after removing seed is squeezed the juice, is centrifuged, is taken supernatant, will
Supernatant is with after the Flat Membrane vacuum filtration in 0.3um aperture, and choosing molecular cut off is 6000 roads
You flat membrane ultrafiltration 80min, then be concentrated in vacuo to Cit mass concentration and be
0.2mg/mL, obtains ultrafiltrate；
2) upper prop wash-out: the regulation of ultrafiltrate pH value is obtained upper prop liquid to 1.5, upper prop liquid is led to
Enter the HD-8 type cationic ion-exchange resin exchange adsorption citrulling that loadings is 25ml, cross post stream
Speed is 5.4BV/h, in efflux Cit mass concentration be adsorb during 0.2mg/mL complete,
With the ammoniacal liquor wash-out that molar concentration is 0.8mol/L, elution flow rate is 5.4BV/h, elutes terminal
It is negative for eluate ninhydrin reaction, collects eluent；
3) decompression distillation: by eluent the 2/3 of vacuum distillation apparatus distillation and concentration to original volume
After inspissated juice；
4) crystallization: being crystallized by inspissated juice absolute ethyl alcohol, crystalline solid slowly separates out to nodeless mesh body
Being terminal during precipitation, the water that crystal quality is 2.5 times of crystal mass after filtration dissolves, then
Repeat to crystallize 2 times with absolute ethyl alcohol, after freeze-drying, obtain Cit crystal, anhydrous second used
Alcohol is 5:1 with the volume ratio of inspissated juice；
Step 2) to the step of cationic ion-exchange resin pretreatment be before: by cation exchange tree
Fat is placed in plastic containers, rinses with clear water, and be soaked in water resin 24h so that it is fully expands,
Then cationic ion-exchange resin is loaded in post, with the 4% of cationic ion-exchange resin volume 6 times
HCl flows through resin bed with the speed of 1mL/min, repeatedly rinses 5 times；The most again with water from upper and
Lower washing resin, until efflux pH is 5；Again with cationic ion-exchange resin volume 4 times 4%
NaOH solution flow through resin bed with the speed of 1mL/min, being then washed to pH is 9, then
Tree is flow through with the speed of 1mL/min with the HCl solution of the 4% of 4 times of cationic ion-exchange resin volumes
Lipid layer, being then washed to pH is 5, without Cl-?.
In one seed melon, the preparation method of Cit effervescent tablet, comprises the steps:
1) Cit 35g, citric acid 17g, mannitol 10g, Sucralose 2g, sweet is taken
Synanthrin glycosides 0.5g, mass concentration are the PVP-k of 90%30Ethanol solution 6g directly makes after mixing
Become granulates, 47 DEG C of dry 3.5h；
2) take sodium acid carbonate 14g, mannitol 16g, mass concentration are the PVP-k of 20%30Ethanol
Solution 9g, is directly prepared into alkali particle, 35 DEG C of dry 12min after mixing；
3) lemon extract 0.6g will be sprayed into after dried granulates, the whole grain of alkali particle, do for 42 DEG C
After dry 0.8h, add 2.5g Macrogol 6000, be mixed evenly, compressing tablet, L-melon
Propylhomoserin effervescent tablet.
Effervescent tablet preparation is temperature required is 30 DEG C, and relative humidity is 43%.
The inspection of effervescent tablet finished product: carry out checking test according to single factor test and orthogonal experiments,
Prepare 3 batches of Cit effervescent tablets, and it is carried out quality examination, when index is respectively disintegrated
Limit, pH value, mouthfeel, hardness and friability.Obtained Cit effervescent tablet is faint yellow
Circular tablet, any surface finish is complete, and tablet weight variation meets regulation, as shown in table 1, average pH
Value is 5.85, sour and sweet palatability, Mean disintegration time 55s, and average hardness is 53N, friability 0.58%,
Result show determined by more excellent technics comparing stable.
Each desired value is tested in table 1 checking
Finally illustrating, above example is only the several exemplary in the present invention, in order to
Technical scheme being described and unrestricted, those of ordinary skill in the art can be to this
Bright technical scheme is modified or equivalent, without deviating from the ancestor of technical solution of the present invention
Purport and scope, it all should be contained in the middle of scope of the presently claimed invention.
Claims (10)
1. the extracting method of Cit in a seed melon, it is characterised in that comprise the steps:
1) ultrafiltrate is prepared: the seed melon melon pulp after removing seed is squeezed the juice, is centrifuged, is taken supernatant, will
Ultrafiltration after supernatant micro-filtrate membrane filtration, then concentrate, obtain ultrafiltrate；
2) upper prop wash-out: by ultrafiltrate pH value to 1.0-2.0, obtain upper prop liquid, upper prop liquid is led to
Enter cationic ion-exchange resin exchange adsorption citrulling, when in detection efflux, Cit quality is dense
Degree is with when in ultrafiltrate, Cit mass concentration is identical, and exchange adsorption is complete, then uses ammoniacal liquor
As eluant, eluent, eluting, wash-out terminal is eluate ninhydrin reaction for feminine gender, collects
Eluent；
3) decompression distillation: obtain inspissated juice after the distillation and concentration that reduced pressure by eluent；
4) crystallization: inspissated juice absolute ethyl alcohol is crystallized, repeats crystallization 2-3 time, freeze-drying
After Cit crystal.
Extracting method the most according to claim 1, it is characterised in that described microfiltration membranes is
The Flat Membrane in 0.1-0.3um aperture, it is that 5000-7000 is daltonian that molecular cut off is chosen in ultrafiltration
Flat Membrane, the ultrafiltration time is 20-80min；
In described ultrafiltrate, Cit mass concentration is 0.2-4.0mg/mL.
Extracting method the most according to claim 1, it is characterised in that described cation is handed over
Changing resin is 001 × 7 type, HD-8 type or 732 types；
The column flow rate of crossing of described upper prop liquid is 3.6-7.2BV/h, the use of described cationic ion-exchange resin
Amount is 20-25ml；
The volume of described inspissated juice is the 1/5-2/3 of effluent volume；
Described inspissated juice and volume ratio 1:3-5 of absolute ethyl alcohol.
Extracting method the most according to claim 1, it is characterised in that rubbing of described ammoniacal liquor
Your concentration is 0.6-0.9mol/L, and elution flow rate is 3.6-7.2BV/h.
Extracting method the most according to claim 1, it is characterised in that described step 2)
The most also include the step to cationic ion-exchange resin pretreatment: be placed in by cationic ion-exchange resin
In plastic containers, rinsing with clear water, be soaked in water resin 12-24h so that it is fully expands,
Then cationic ion-exchange resin is loaded in post, with the 4% of cationic ion-exchange resin volume 3-6 times
HCl flow through resin bed with the speed of 1mL/min, repeatedly rinse 3 to 5 times；Use the most again
Water washing resin from top to bottom, until efflux pH is 3-5；Use cationic ion-exchange resin body again
The NaOH solution of long-pending 2-4 times 4% flows through resin bed with the speed of 1mL/min, is then washed to
PH is 8-9, then with the 4% of 2-4 times of cationic ion-exchange resin volume HCl solution with 1mL/min
Speed flow through resin bed, being then washed to pH is 3-5, without Cl-?.
6. a Cit, it is characterised in that described in any one of claim 1-5
Extracting method prepares.
7. the composition for effervescent tablet, it is characterised in that include the group of following weight portion
Point:
Cit 25-35 part, citric acid 17-21 part, mannitol 10-14 part, Sucralose
2-4 part, steviol glycoside 0.1-0.5 part, PVP-k30Ethanol solution A 4-6 part；
Sodium acid carbonate 14-17 part, mannitol 16-20 part, PVP-k30Ethanol B solution 5-9 part；
Lemon extract 0.6-1.0 part, Macrogol 6000 1.8-2.5 part；
Described Cit is selected from Cit described in claim 5；
Described PVP-k30Ethanol solution A be mass concentration be the PVP-k of 90%30Ethanol solution,
Described PVP-k30Ethanol B solution be mass concentration be the PVP-k of 20%30Ethanol solution.
8. use the method that the composition described in claim 7 prepares effervescent tablet, it is characterised in that
Comprise the steps:
1) by Cit, citric acid, mannitol, Sucralose, steviol glycoside, PVP-k30
Ethanol solution A is directly prepared into granulates after mixing, and is then dried granulates；
2) by sodium acid carbonate, mannitol and PVP-k30Ethanol B solution is directly made after mixing
Become alkali particle, be then dried alkali particle；
3) after granulates and the whole grain of alkali particle, spray into lemon extract, add polyethylene glycol after drying
6000, be mixed evenly, compressing tablet, effervescent tablet.
Method the most according to claim 8, it is characterised in that described when preparing effervescent tablet
Temperature required for 18-30 DEG C, relative humidity is 30-48%.
Method the most according to claim 8, it is characterised in that described step 1) in dry
Dry temperature is 42-47 DEG C, and the time being dried is 1.5-3.5h；Described step 2) in be dried
Temperature is 35-42 DEG C, and the time being dried is 8-12min；Described step 3) in be dried temperature
For 38-42 DEG C, the time being dried is 0.8-1.2h.
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Cited By (3)
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| CN106430644A (en) * | 2016-10-09 | 2017-02-22 | 华南理工大学 | Edible descaling agent and scale inhibition sintered carbon rod prepared from same |
| CN112608254A (en) * | 2020-12-29 | 2021-04-06 | 南通紫琅生物医药科技有限公司 | Method for preparing L-citrulline |
| WO2024020843A1 (en) * | 2022-07-27 | 2024-02-01 | 中国科学院广州生物医药与健康研究院 | Use of citrulline or pharmaceutically acceptable salt thereof in preparation of medicament for improving immunity or preventing or treating anxiety disorder |
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